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SUMMARY The construction and method of use of an inexpensive spray‐freezing device are described.

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Lately novel strategies to enhance the sensing properties on iron oxide have been proposed to achieve high performance gas sensors for acetone detection. In this working report, the synthesis of iron-glycerate (Fe-Gly) using glycerol to combine with Fe3+ is first presented. Depending on the thermal treatment, this compound can evolve into γ-Fe2O3, α/γ-Fe2O3 and α-Fe2O3. α/γ-Fe2O3 shows better sensing performance as far as acetone detection is concerned. Using the dual phases of α/γ-Fe2O3 as a fundamental building block, their sensing properties were further improved using Ni doping and Ru nanoparticles functionalization. The high response and selectivity to acetone detection was ascribed to the synergistic effects of unique nanosheets, mixed phases, rich oxygen vacancies and excellent catalytic activity of Ru nanoparticles. Graphical abstract